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A kind of concave structure single crystal graphene and preparation method thereof

A single-crystal graphene, concave technology, applied in the field of controllable preparation of single-crystal graphene, can solve problems such as high cost, and achieve the effects of low cost, simple preparation method and good application prospect

Active Publication Date: 2019-09-10
WUHAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Among them, the graphene with the target structure obtained by photolithography needs to go through steps such as spin coating, mask making, photolithography, and adhesive removal, which is very expensive.

Method used

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  • A kind of concave structure single crystal graphene and preparation method thereof
  • A kind of concave structure single crystal graphene and preparation method thereof
  • A kind of concave structure single crystal graphene and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] A kind of concave structure monocrystalline graphene, its preparation method comprises the steps:

[0025] 1) Cut copper foil with an area of ​​2cm×2cm, and use acetic acid (purity: 99.5wt%) and acetone (concentration: 99.5wt%) to ultrasonically clean the copper foil for 20 minutes; put the cleaned copper foil into a quartz tube, and the quartz The diameter of the tube is 6cm, the length is 100cm, and 500sccm of Ar is passed into it for 30 minutes to ensure that the air in the quartz tube is exhausted, and then 50sccm of H is passed into it at the same time. 2 , rise to 1050°C at a rate of 15°C / min, hold for 90min (annealing), turn off H 2 ;

[0026] 2) Keep the Ar gas flow in step 1) to exhaust the H in the quartz tube 2 , and then into 3sccm O 2 Carry out pre-oxidation treatment, keep for 5min, the oxidation temperature is 1050°C, turn off O 2 ; Keep the flow of Ar in step 2) constant, H 2 The flow rate is increased to 300sccm, and 1sccm of CH is introduced 4 , ...

Embodiment 2

[0031] A kind of concave structure monocrystalline graphene, its preparation method comprises the steps:

[0032] 1) Cut copper foil with an area of ​​2cm×2cm, and use acetic acid (purity: 99.5wt%) and acetone (concentration: 99.5wt%) to ultrasonically clean the copper foil for 30 minutes; put the cleaned copper foil into a quartz tube, and the quartz The diameter of the tube is 6cm, the length is 100cm, and 750sccm of Ar is passed into it for 30 minutes to ensure that the air in the quartz tube is exhausted, and then 75sccm of H is passed into it at the same time. 2 , rise to 1065°C at a rate of 15°C / min, hold for 100min, turn off H 2 (annealing);

[0033] 2) Keep the Ar gas flow in step 1) to exhaust the H in the quartz tube 2 , and then into 4sccm O 2 , keep 7min, oxidation temperature 1065℃, close O 2 ; Keep the flow of Ar in step 2) constant, H 2 The flow rate is increased to 400sccm, and 1.2sccm of CH4 , perform chemical vapor deposition at 1065°C, and keep growing ...

Embodiment 3

[0037] A kind of concave structure monocrystalline graphene, its preparation method comprises the steps:

[0038] 1) Cut copper foil with an area of ​​2cm×2cm, and use acetic acid (purity: 99.5wt%) and acetone (concentration: 99.5wt%) to ultrasonically clean the copper foil for 40 minutes; put the cleaned copper foil into a quartz tube, and the quartz The diameter of the tube is 6cm, the length is 100cm, and 1000sccm of Ar is passed into it for 30 minutes to ensure that the air in the quartz tube is exhausted, and then 100sccm of H is passed into it at the same time 2 , rise to 1080°C at a rate of 15°C / min, hold for 120min (annealing), turn off H 2 ;

[0039] 2) Keep the Ar gas flow in step 1) to exhaust the H in the quartz tube 2 , and then into 5sccm of O 2 Carry out pre-oxidation treatment, keep for 10min, the oxidation temperature is 1080°C, turn off O 2 ; Keep the flow of Ar in step 2) constant, H 2 The flow rate is increased to 500sccm, and 1.5sccm of CH is introduc...

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Abstract

The invention discloses a preparation method of concave structure monocrystalline graphene. The method comprises the following steps: 1, carrying out ultrasonic cleaning on a copper foil substrate by using acetic acid and acetone, and carrying out pre-annealing treatment; 2, pre-oxidizing the annealed copper foil substrate; and 3, carrying out chemical vapor deposition on the pre-oxidized copper foil through adopting a chemical vapor deposition technology, and cooling the deposited copper foil to obtain the concave structure monocrystalline graphene. The preparation method has the advantages of simplicity, convenience in operation, good repeatability, reparation of the concave (internal single layer and external double layers) structure monocrystalline graphene through controlling reaction atmosphere and low cost, and the concave structure monocrystalline graphene has very good application prospect in the fields of optical and microwave diodes and sensors.

Description

technical field [0001] The invention relates to a single-crystal graphene with a concave structure and a preparation method thereof, in particular to a controllable preparation of single-crystal graphene with a single-layer peripheral double-layer structure in the middle. Background technique [0002] Since 2004, people have made great breakthroughs in the research on the properties and applications of graphene, and the corresponding graphene preparation technology is also advancing rapidly. It is important to find a fast and cheap way to prepare high-quality graphene. The focus of all graphene researchers. So far, people have developed mechanical exfoliation method, silicon carbide epitaxy method, liquid phase exfoliation method, redox method, chemical vapor deposition method and bottom-up synthesis method and other preparation methods. These methods have their own advantages and are suitable for different occasions, among which chemical vapor deposition is considered to b...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B32/186C30B29/02C30B25/00C30B29/64
Inventor 涂溶张翅腾飞章嵩张联盟
Owner WUHAN UNIV OF TECH
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